反应详情

Hydrogen chloride in dioxane (4N, 7 mL, 28 mmol) was added to a suspension of 199 mg (0.474 mmol) of the product of Example 20G in 1 mL dioxane. After stirring 45 minutes, the mixture was quenched with 3N NaOH solution, then diluted with EtOAc and poured into water. The separated organic phase was washed with brine, dried (Na2SO4), filtered and concentrated under reduced pressure. The crude product was triturated with Et2O and the solid was collected by vacuum filtration. The result was 92 mg (61%) of the title compound as a pale pink solid. 1H NMR (DMSO-d6) δ 9.02 (br s, 1H), 7.57 (d, J=7.1 Hz, 1H), 7.45 (d, J=8.1 Hz, 2H), 7.28 (s, 1H), 7.23 (d, J=8.1 Hz, 2H), 7.08 (t, J=7.8 Hz, 1H), 6.83 (d, J=7.1 Hz, 1H), 3.05-2.70 (m, 4H), 2.31 (m, 4H), 1.85 (m, 3H), 1.42 (m, 1H); MS (ESI+) m/z 320 (M+H)+.

1. customthe mixture was quenched with 3N NaOH solution
2. additiondiluted with EtOAc
3. additionpoured into water
4. washThe separated organic phase was washed with brine
5. dry with materialdried (Na2SO4)
6. filtrationfiltered
7. concentrationconcentrated under reduced pressure
8. customThe crude product was triturated with Et2O
9. filtrationthe solid was collected by vacuum filtration